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用于定量测定人血浆中曲克芦丁的液相色谱/串联质谱分析法

Liquid chromatography/tandem mass spectrometry assay for the quantification of troxerutin in human plasma.

作者信息

Liu Fei, Xu Yu, Rui Lei, Gao Shu, Dong Haijun, Guo Qingxiang

机构信息

Department of Chemistry, University of Science and Technology of China, Hefei 230026, China.

出版信息

Rapid Commun Mass Spectrom. 2006;20(23):3522-6. doi: 10.1002/rcm.2764.

Abstract

A simple, rapid, sensitive and specific liquid chromatography/tandem mass spectrometry method was developed and validated to quantify troxerutin in human plasma. The analyte and rutin, used as the internal standard, were analyzed on a Phenomenex Synergi Fusion RP column interfaced with a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. Acetonitrile/water (20:80 v/v) was used as the isocratic mobile phase, with 0.1% formic acid in water. A simple sample preparation method of protein precipitation with perchloric acid was employed. The assay was linear over the concentration range 31.25-4000 pg/mL. Correlation coefficients generated by linear regression with a 1/x(2) weighting factor ranged from 0.9991 to 0.9996. The intra- and inter-day precision over the entire concentration range were less than 12.28%. The method was successfully applied to a pharmacokinetic study after oral administration of a 300 mg troxerutin drop pill to 18 healthy volunteers.

摘要

建立并验证了一种简单、快速、灵敏且特异的液相色谱/串联质谱法,用于定量测定人血浆中的曲克芦丁。以芦丁作为内标物,在配备了电喷雾正离子源的三重四极杆串联质谱仪的Phenomenex Synergi Fusion RP色谱柱上对分析物和内标物进行分析。乙腈/水(20:80 v/v)作为等度流动相,水相中含有0.1%的甲酸。采用了用高氯酸沉淀蛋白质的简单样品制备方法。该测定法在31.25 - 4000 pg/mL的浓度范围内呈线性。通过具有1/x(2)加权因子的线性回归生成的相关系数在0.9991至0.9996之间。在整个浓度范围内,日内和日间精密度均小于12.28%。该方法成功应用于18名健康志愿者口服300 mg曲克芦丁滴丸后的药代动力学研究。

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